U‐PVC gelation level assessment, part 2: Optimization of the differential scanning calorimetry technique

Differential scanning calorimetry (DSC) is one of the best techniques for assessing PVC gelation level. Thus, it is of great interest to understand and optimize the different aspects of the DSC method. In the present study, DSC experiments were carried out on PVC dryblend samples that were previously heat‐treated at different temperatures. Practical aspects such as sample preparation, heating rate, and ending temperature are described. Then, the obtained DSC patterns are compared and analyzed to clarify the origin of the measured events. The effects of PVC reprocessing on DSC patterns are presented, as well as the effects of heterogeneity issues (i) at the scale of a PVC window profile and (ii) at the scale of a PVC DSC sample. The method used for the determination of the gelation level is then analyzed. The choice of the integration limits that strongly affect the melting enthalpy values is discussed. Different ways of calculating the gelation level, including the conventional definition involving the ratio A / A + B as well as new approaches, are proposed. J. VINYL. ADDIT. TECHNOL. 12:108–114, 2006.